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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Formation and Decomposition of Iron Nitrides Observed by in situ Powder Neutron Diffraction and Thermal Analysis
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Formation and Decomposition of Iron Nitrides Observed by in situ Powder Neutron Diffraction and Thermal Analysis

机译：原位粉末中子衍射和热分析观察到的氮化铁的形成和分解

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摘要

In order to gain more information on the formation and decomposition behavior of various iron nitrides from different starting materials in situ neutron diffraction and thermal analysis under application of different gas atmospheres and heating rates were carried out. The following phases were observed during these investigations:crystalline α-Fe, γ-FeNz, γ'-Fe_4N_y, ε-Fe_3N_(1+x), ζ-Fe_2N, FeCl_2, [Fe(NH_3)_6]Cl_2, Fe(NH_3)_2Cl_2, and amorphous Fe(NH_3)Cl_2. In situ neutron diffraction data were collected in high quality, due to an optimized experimental setup with a time resolution of two minutes on D20 (Institut Laue-Langevin) allowing for detailed Rietveld analyses. For all phase transitions, decomposition and formation temperatures a strong dependency from the heating rate, thermal history of the sample, gas flow conditions, and particle size exists. The nitrogen contents observed during thermal decomposition of ζ-Fe_2N were related to the binary phase diagram Fe-N. At low temperatures (<400 ℃) ε- and ζ-phase are non-equilibrated. However, through annealing equilibrium state is reached. For γ'-Fe_4N_y formed in situ at higher temperatures an expansion of the homogeneity range towards lower nitrogen content is observed above 600 ℃. For the formation of ε-Fe_3N_(1+x) from FeCl_2 and NH_3 a previously proposed reaction sequence involving different ammoniates was confirmed. This reaction occurs via formation of amorphous Fe(NH_3)Cl_2. The therein observed in situ formed ammoniates were additionally characterized by IR spectroscopy.
机译：为了获得更多关于不同原料形成的各种氮化铁的形成和分解行为的信息，在不同的气体气氛和加热速率下进行了中子衍射和热分析。在这些研究中观察到以下相：晶体α-Fe，γ-FeNz，γ'-Fe_4N_y，ε-Fe_3N_（1 + x），ζ-Fe_2N，FeCl_2，[Fe（NH_3）_6] Cl_2，Fe（NH_3 ）_2Cl_2和无定形Fe（NH_3）Cl_2。由于在D20（Institut Laue-Langevin）上进行了两分钟时间分辨率的优化实验设置，可以进行高质量的原位中子衍射数据，从而可以进行详细的Rietveld分析。对于所有相变，分解和形成温度，都强烈依赖于加热速率，样品的热历史，气体流动条件和粒径。 ζ-Fe_2N热分解过程中观察到的氮含量与二元相图Fe-N有关。在低温（<400℃）下，ε相和ζ相不平衡。但是，通过退火达到平衡状态。对于在较高温度下原位形成的γ'-Fe_4N_y，在600℃以上观察到均匀范围向较低的氮含量扩展。为了由FeCl_2和NH_3形成ε-Fe_3N_（1 + x），证实了先前提出的涉及不同氨化物的反应顺序。该反应通过形成无定形的Fe（NH_3）Cl_2而发生。现场观察到的氨形成的氨化物还通过红外光谱表征。

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